EP3522855A1 - Process for manufacture of non-aqueous oral care compositions - Google Patents

Process for manufacture of non-aqueous oral care compositions

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Publication number
EP3522855A1
EP3522855A1 EP17780360.8A EP17780360A EP3522855A1 EP 3522855 A1 EP3522855 A1 EP 3522855A1 EP 17780360 A EP17780360 A EP 17780360A EP 3522855 A1 EP3522855 A1 EP 3522855A1
Authority
EP
European Patent Office
Prior art keywords
sodium
phosphate
surfactant
polyol
process according
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP17780360.8A
Other languages
German (de)
French (fr)
Other versions
EP3522855B1 (en
Inventor
Richard Aaron FORREST
Brian Joseph Groves
Pierre Starck
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Unilever Global IP Ltd
Unilever IP Holdings BV
Original Assignee
Unilever PLC
Unilever NV
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Filing date
Publication date
Application filed by Unilever PLC, Unilever NV filed Critical Unilever PLC
Publication of EP3522855A1 publication Critical patent/EP3522855A1/en
Application granted granted Critical
Publication of EP3522855B1 publication Critical patent/EP3522855B1/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34—Alcohols
    • A61K8/345—Alcohols containing more than one hydroxy group
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/24—Phosphorous; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/46—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur
    • A61K8/463—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur containing sulfuric acid derivatives, e.g. sodium lauryl sulfate
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/46—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur
    • A61K8/466—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur containing sulfonic acid derivatives; Salts
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
    • A61K2800/30—Characterized by the absence of a particular group of ingredients
    • A61K2800/31—Anhydrous
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/48—Thickener, Thickening system

Definitions

  • the present invention is concerned with a process for preparing non-aqueous oral care compositions.
  • Oral care compositions such as dentifrices typically contain dentally acceptable abrasive, humectant, water, and water-soluble polymer which serves as a thickener and binder for the ingredients.
  • dentally acceptable abrasive, humectant, water, and water-soluble polymer which serves as a thickener and binder for the ingredients.
  • other ingredients such as flavours, sweeteners,
  • preservatives and fluoride are also utilized at low levels.
  • non-aqueous compositions incorporating the above ingredients can be difficult to conduct in a manner that produces a toothpaste with sensory properties that are acceptable to the consumer.
  • non-aquous compositions require structurants and process for incorporating these structurants can be difficult to perform in a manner that gives consistent rheological properties.
  • WO96/03108 describes a non-aqueous dentifrice composition
  • a non-aqueous dentifrice composition comprising a carboxyvinyl polymer, a humectant, a polyethylene glycol and a dentally acceptable abrasive.
  • the carboxyvinyl polymer is used to thicken the humectant materials and provide the necessary rheology in order to suspend any required abrasive material.
  • WO96/03108 is that they do not behave Theologically like a typical aqueous dentifrice. This problem is observed both during manufacture and during use by the consumer. It has led to manufacturing difficulties and reduced acceptance amongst consumers.
  • the present invention relates to a process for producing non aqueous toothpastes with good sensory rheological parameters and without the need for further thickeners.
  • the present invention provides a process for manufacturing a non-aqueous composition
  • a process for manufacturing a non-aqueous composition comprising the following steps: i) addition of an anionic surfactant selected form the group consisting of, alfa olefin sulfonate, lauryl phosphate, sodium coco sulphate, sodium methyl cocoyl taurate, sodium methyl oleoyl taurate, sodium lauryl sulphate, sodium cocoyl isethionate, disodium lauryl sulfosuccinate, to a polyol at a temperature such that the surfactant completely dissolves in the polyol followed by; ii) addition of a alkali metal phosphate salt; iii) cooling of the mix to a temperature below the solubility point of the surfactant in polyol, the cooling resulting in a structured mix, in which the weight ratio of phosphate to surfactant is from 1.1 :1 to 10:1 .
  • surfactant crystals selected form the group consisting of, alfa olefin sulfonate, lauryl phosphate, sodium coco sulphate, sodium methyl cocoyl taurate, sodium methyl oleoyl taurate, sodium lauryl sulphate, sodium cocoyl isethionate, disodium
  • lauryl sulfosuccinate to structure a non-aqueous paste comprising polyol and alkali metal phosphate.
  • the present invention relates to a process for manufacturing a non-aqueous composition
  • the surfactant is heated in the polyol to a temperature of 60°C or above.
  • the composition comprises a perfume and/or flavouring
  • they are added after the mix is cooled to a temperature below the solubility point of the surfactant in the polyol.
  • the perfume or flavouring is added to the mix after step iii) (cooling of the mix to a temperature below the solubility point of the surfactant in polyol) at a temperature of 45°C or below.
  • the composition of the invention is non-aqueous. By “non-aqueous" it is generally meant that water is not deliberately added to the composition in any significant quantity.
  • non-aqueous does not mean that small amounts of water cannot be present, for example as a consequence of its association with hygroscopic raw materials. Accordingly, for the purposes of this invention, the term “non-aqueous” generally means that water is present in an amount no greater than about 5%, more preferably no greater than about 3% more preferably no greater than 1 % by weight based on the total weight of the composition.
  • compositions according to the invention comprises a polyol.
  • Preferred polyols include organic polyols having 3 or more hydroxyl groups in the molecule (hereinafter termed "organic polyols"). Examples of such materials include glycerol, sorbitol, xylitol, mannitol, lactitol, maltitol, erythritol, and hydrogenated partially hydrolyzed polysaccharides.
  • the most preferred organic polyol is glycerol. Mixtures of any of the above described materials may also be used.
  • the level of polyol will depend on the particular type chosen, but generally ranges from about 20 to 90% by weight based on the total weight of the composition, the amount of organic polyol suitably ranges from 35 to 75%, more preferably from 45 to 70% by total weight organic polyol based on the total weight of the composition.
  • the composition of the invention is organic polyol-based.
  • organic polyol-based means that the composition is not oil-based or water-based, but instead, organic polyols (as defined above) are a principal component in the composition.
  • principal component is meant that the organic polyols (as defined above) when taken together, make up a higher portion of the composition's weight than any other compound.
  • the composition of the invention is glycerol-based (i.e.
  • glycerol makes up a higher portion of the composition's weight than any other compound) and contains from 45 to 70% by weight glycerol based on the total weight of the composition.
  • compositions of the invention comprise an anionic a surfactant.
  • the anionic surfactant is selected form the group consisting of, alfa olefin sulfonate, lauryl phosphate, sodium coco sulphate, sodium methyl cocoyi taurate, sodium methyl oleoyl taurate, sodium lauryl sulphate, sodium cocoyi isethionate, disodium lauryl sulfosuccinate and mixtures thereof. More preferably the anionic surfactant is selected from the group consisting of sodium coco sulphate, sodium methyl cocoyi taurate sodium lauryl sulphate (SLS) and mixtures thereof.
  • the level of anionic surfactant is from in an amount of from 0.2 to 5 wt%, more preferably form 1 to 3 wt% of the total composition.
  • composition of the invention comprise an alkali metal phosphate salt.
  • the phosphate salt used is one which results in an oral care composition (i.e., combined composition if a dual phase product) having a pH from 5.5 to 8, preferably from 6 to 7.5, and most preferably, about neutral.
  • Suitable phosphate salts include sodium dihydrogen phosphate, disodium hydrogen phosphate, sodium pyrophosphate, tetrasodium pyrophosphate, sodium tripolyphosphate, sodium hexametaphosphate, potassium dihydrogenphosphate, trisodium phosphate, tripotassium phosphate and mixtures thereof.
  • the phosphate salt used is trisodium phosphate and monosodium dihydrogen phosphate, more preferably at a trisodium phosphate to monosodium dihydrogen phosphate weight ratio of 1 :4 to 4:1 , most preferably, from 1 :2 to 2:1 , including all ratios subsumed therein.
  • the amount phosphate source(s) (e.g. trisodium phosphate and sodium dihydrogen phosphate) in the composition of this invention typically ranges from 1 to 15wt%, preferably from 2 to 10wt%, more preferably from 3 to 8% of the total composition. Thickening Agent
  • the liquid continuous phase of the composition of the invention is preferably free of thickening agent.
  • thickening agent include carboxyvinyl polymers.
  • the composition of the invention is typically in the form of a dentifrice or serum.
  • dentifrice denotes a formulation which are used to clean the surfaces of the oral cavity.
  • the dentifrice is an oral composition that is not intentionally swallowed for purposes of systemic administration of therapeutic agents, but is retained in the oral cavity for a sufficient time to contact substantially all of the dental surfaces and/or mucosal tissues for purposes of oral activity.
  • the dentifrice is suitable for application with a toothbrush and is rinsed off after use.
  • the dentifrice is in the form of an extrudable semi-solid such as a cream, paste or gel (or mixture thereof).
  • a dentifrice composition according to the invention will generally contain further ingredients to enhance performance and/or consumer acceptability.
  • the dentifrice may comprise other abrasive materials (in addition to the abrasive amorphous silica particles described above).
  • Such other abrasive materials will generally be present in an amount of from 3 to 75% by weight based on the total weight of the dentifrice.
  • Suitable other abrasive materials include other abrasive silicas (i.e.
  • composition of the invention is particularly suitable as a vehicle for oral care actives which may be physically or chemically incompatible with water, or which may function less efficiently in an aqueous environment.
  • oral care actives which may be included in the compositions of the invention include: fluoride sources such as sodium fluoride, stannous fluoride, sodium
  • monofluorophosphate zinc ammonium fluoride, tin ammonium fluoride, calcium fluoride, cobalt ammonium fluoride and mixtures thereof; plant-derivable antioxidants such as flavonoid, catechin, polyphenol, and tannin compounds and mixtures thereof; antioxidant vitamins such as tocopherols and/or derivatives thereof, ascorbic acid and/or derivatives thereof and mixtures thereof.
  • oral care actives for inclusion in the compositions of the invention include agents for the remineralisation of teeth.
  • remineralisation in the context of the present invention means the in situ generation of hydroxyapatite on teeth.
  • a specific example of a suitable agent for the remineralisation of teeth is a mixture of a calcium source and a phosphate source which, when delivered to the teeth results in the in situ generation of hydroxyapatite on teeth.
  • remineralising calcium sources include, for example, calcium phosphate, calcium gluconate, calcium oxide, calcium lactate, calcium glycerophosphate, calcium carbonate, calcium hydroxide, calcium sulphate, calcium carboxymethyl cellulose, calcium alginate, calcium salts of citric acid, calcium silicate and mixtures thereof.
  • the remineralising calcium source is calcium silicate.
  • the amount of remineralising calcium source(s) (e.g. calcium silicate) in the composition of the invention typically ranges from 1 to 30%, preferably from 5 to 20% by total weight remineralising calcium source based on the total weight of the oral care composition.
  • compositions of the present invention may also contain further optional ingredients customary in the art such as anticaries agents, anticalculus agents, buffers, flavouring agents, sweetening agents, colouring agents, opacifying agents, preservatives, antisensitivity agents, antimicrobial agents and the like.
  • a whitening agent Preferably the composition comprising a whitening agent. Suitable whitening agents comprise titanium dioxide, mica and blue dyes/pigments. Mixtures of whitening agents may be used.
  • a toothpaste was manufactured by the following steps: i) Addition of an anionic surfactant to a polyol and heating to a temperature such that the surfactant completely dissolves in the polyol followed by; ii) addition of other ingredients with the exception of alkali metal salt (phosphate), perfume and flavours; iii) addition of alkali metal salt (phosphate) and allow time for solution to disperse; iv) optionally; v) cooling of the mix to a temperature below the solubility point of the surfactant in polyol; vi) addition of perfumes and flavour; vii) cooling resulting in a structured mix. Constant Shear is present from the start of the process to the end. So the shear does not impact upon the invention but will help surfactants and metal salts to dissolve but their dissolution is mostly influence by temperature.
  • the invention is further illustrated with reference to the following, non-limiting Examples.
  • Unstructured Formulation eg surfactant introduced late or after the source of phosphate
  • Table 2 Examples of Unstructured Formulation (eg surfactant introduced late or after the source of phosphate) are shown in Table 2.
  • Viscosity Viscosity Viscosity Yield Stress Pa.s) (Pa.s) (Pa.s) (Pa) at shear rate at shear rate at shear rate
  • SMCT late unstructured Products made according to the invention do not need any extra structuring technologies (such as polymers) in them as these products hold their structure until a certain stress is applied to them - They typically exhibit a yield stress and behave as a toothpaste.

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Epidemiology (AREA)
  • Birds (AREA)
  • Emergency Medicine (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Cosmetics (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

Process for manufacturing a non-aqueous composition comprising the following steps: i) addition of an anionic surfactant to a polyol at a temperature such that the surfactant completely dissolves in the polyol followed by; ii) addition of a alkali metal salt; cooling of the mix to a temperature below the solubility point of the surfactant in polyol, the cooling resulting in a structured mix.

Description

PROCESS FOR MANUFACTURE OF NON-AQUEOUS ORAL CARE COMPOSITIONS
Field of the Invention
The present invention is concerned with a process for preparing non-aqueous oral care compositions.
Background of the Invention
Oral care compositions such as dentifrices typically contain dentally acceptable abrasive, humectant, water, and water-soluble polymer which serves as a thickener and binder for the ingredients. A variety of other ingredients such as flavours, sweeteners,
preservatives and fluoride are also utilized at low levels.
However the processes for preparing non-aqueous compositions incorporating the above ingredients can be difficult to conduct in a manner that produces a toothpaste with sensory properties that are acceptable to the consumer. Furthermore many non-aquous compositions require structurants and process for incorporating these structurants can be difficult to perform in a manner that gives consistent rheological properties.
WO96/03108 describes a non-aqueous dentifrice composition comprising a carboxyvinyl polymer, a humectant, a polyethylene glycol and a dentally acceptable abrasive. The carboxyvinyl polymer is used to thicken the humectant materials and provide the necessary rheology in order to suspend any required abrasive material.
A further problem with non-aqueous formulations such as those disclosed in
WO96/03108 is that they do not behave Theologically like a typical aqueous dentifrice. This problem is observed both during manufacture and during use by the consumer. It has led to manufacturing difficulties and reduced acceptance amongst consumers. The present invention relates to a process for producing non aqueous toothpastes with good sensory rheological parameters and without the need for further thickeners.
Products made using these processing parameters are stable on storage.
Summary of the Invention
The present invention provides a process for manufacturing a non-aqueous composition comprising the following steps: i) addition of an anionic surfactant selected form the group consisting of, alfa olefin sulfonate, lauryl phosphate, sodium coco sulphate, sodium methyl cocoyl taurate, sodium methyl oleoyl taurate, sodium lauryl sulphate, sodium cocoyl isethionate, disodium lauryl sulfosuccinate, to a polyol at a temperature such that the surfactant completely dissolves in the polyol followed by; ii) addition of a alkali metal phosphate salt; iii) cooling of the mix to a temperature below the solubility point of the surfactant in polyol, the cooling resulting in a structured mix, in which the weight ratio of phosphate to surfactant is from 1.1 :1 to 10:1 .
Use of surfactant crystals selected form the group consisting of, alfa olefin sulfonate, lauryl phosphate, sodium coco sulphate, sodium methyl cocoyl taurate, sodium methyl oleoyl taurate, sodium lauryl sulphate, sodium cocoyl isethionate, disodium
lauryl sulfosuccinate, to structure a non-aqueous paste comprising polyol and alkali metal phosphate.
Detailed Description of the Invention
The present invention relates to a process for manufacturing a non-aqueous composition comprising steps of adding an anionic surfactant to a polyol at a temperature such that the surfactant completely dissolves in the polyol. Preferably the surfactant is heated in the polyol to a temperature of 60°C or above.
Preferably if the composition comprises a perfume and/or flavouring, they are added after the mix is cooled to a temperature below the solubility point of the surfactant in the polyol. More preferably the perfume or flavouring is added to the mix after step iii) (cooling of the mix to a temperature below the solubility point of the surfactant in polyol) at a temperature of 45°C or below. The composition of the invention is non-aqueous. By "non-aqueous" it is generally meant that water is not deliberately added to the composition in any significant quantity.
However, the term "non-aqueous" does not mean that small amounts of water cannot be present, for example as a consequence of its association with hygroscopic raw materials. Accordingly, for the purposes of this invention, the term "non-aqueous" generally means that water is present in an amount no greater than about 5%, more preferably no greater than about 3% more preferably no greater than 1 % by weight based on the total weight of the composition. Polyol
Compositions according to the invention comprises a polyol. Preferred polyols include organic polyols having 3 or more hydroxyl groups in the molecule (hereinafter termed "organic polyols"). Examples of such materials include glycerol, sorbitol, xylitol, mannitol, lactitol, maltitol, erythritol, and hydrogenated partially hydrolyzed polysaccharides. The most preferred organic polyol is glycerol. Mixtures of any of the above described materials may also be used.
The level of polyol will depend on the particular type chosen, but generally ranges from about 20 to 90% by weight based on the total weight of the composition, the amount of organic polyol suitably ranges from 35 to 75%, more preferably from 45 to 70% by total weight organic polyol based on the total weight of the composition. Most preferably the composition of the invention is organic polyol-based. In the context of the present invention, the term "organic polyol-based" means that the composition is not oil-based or water-based, but instead, organic polyols (as defined above) are a principal component in the composition. By "principal component" is meant that the organic polyols (as defined above) when taken together, make up a higher portion of the composition's weight than any other compound. Ideally the composition of the invention is glycerol-based (i.e.
glycerol makes up a higher portion of the composition's weight than any other compound) and contains from 45 to 70% by weight glycerol based on the total weight of the composition.
Surfactant
Compositions of the invention comprise an anionic a surfactant.
The anionic surfactant is selected form the group consisting of, alfa olefin sulfonate, lauryl phosphate, sodium coco sulphate, sodium methyl cocoyi taurate, sodium methyl oleoyl taurate, sodium lauryl sulphate, sodium cocoyi isethionate, disodium lauryl sulfosuccinate and mixtures thereof. More preferably the anionic surfactant is selected from the group consisting of sodium coco sulphate, sodium methyl cocoyi taurate sodium lauryl sulphate (SLS) and mixtures thereof.
Preferably the level of anionic surfactant is from in an amount of from 0.2 to 5 wt%, more preferably form 1 to 3 wt% of the total composition.
Alkali Metal Salt
Composition of the invention comprise an alkali metal phosphate salt. In a preferred embodiment, the phosphate salt used is one which results in an oral care composition (i.e., combined composition if a dual phase product) having a pH from 5.5 to 8, preferably from 6 to 7.5, and most preferably, about neutral.
Suitable phosphate salts include sodium dihydrogen phosphate, disodium hydrogen phosphate, sodium pyrophosphate, tetrasodium pyrophosphate, sodium tripolyphosphate, sodium hexametaphosphate, potassium dihydrogenphosphate, trisodium phosphate, tripotassium phosphate and mixtures thereof. Preferably the phosphate salt used is trisodium phosphate and monosodium dihydrogen phosphate, more preferably at a trisodium phosphate to monosodium dihydrogen phosphate weight ratio of 1 :4 to 4:1 , most preferably, from 1 :2 to 2:1 , including all ratios subsumed therein. The amount phosphate source(s) (e.g. trisodium phosphate and sodium dihydrogen phosphate) in the composition of this invention typically ranges from 1 to 15wt%, preferably from 2 to 10wt%, more preferably from 3 to 8% of the total composition. Thickening Agent
The liquid continuous phase of the composition of the invention is preferably free of thickening agent. In the context of the present invention this means that the compositions comprises less than 0.05 wt% of the total composition. Such thickening agents include carboxyvinyl polymers.
Product Form and Optional Ingredients
The composition of the invention is typically in the form of a dentifrice or serum. The term "dentifrice" denotes a formulation which are used to clean the surfaces of the oral cavity. The dentifrice is an oral composition that is not intentionally swallowed for purposes of systemic administration of therapeutic agents, but is retained in the oral cavity for a sufficient time to contact substantially all of the dental surfaces and/or mucosal tissues for purposes of oral activity. Preferably the dentifrice is suitable for application with a toothbrush and is rinsed off after use. Preferably the dentifrice is in the form of an extrudable semi-solid such as a cream, paste or gel (or mixture thereof).
A dentifrice composition according to the invention will generally contain further ingredients to enhance performance and/or consumer acceptability. For example, the dentifrice may comprise other abrasive materials (in addition to the abrasive amorphous silica particles described above). Such other abrasive materials will generally be present in an amount of from 3 to 75% by weight based on the total weight of the dentifrice. Suitable other abrasive materials include other abrasive silicas (i.e. abrasive silicas which are different to the abrasive amorphous silica particles described above), calcium carbonate, dicalcium phosphate, tricalcium phosphate, calcined alumina, sodium and potassium metaphosphate, sodium and potassium pyrophosphates, sodium trimetaphosphate, sodium hexametaphosphate, particulate hydroxyapatite and mixtures thereof. Being non-aqueous, the composition of the invention is particularly suitable as a vehicle for oral care actives which may be physically or chemically incompatible with water, or which may function less efficiently in an aqueous environment.
Specific examples of oral care actives which may be included in the compositions of the invention include: fluoride sources such as sodium fluoride, stannous fluoride, sodium
monofluorophosphate, zinc ammonium fluoride, tin ammonium fluoride, calcium fluoride, cobalt ammonium fluoride and mixtures thereof; plant-derivable antioxidants such as flavonoid, catechin, polyphenol, and tannin compounds and mixtures thereof; antioxidant vitamins such as tocopherols and/or derivatives thereof, ascorbic acid and/or derivatives thereof and mixtures thereof.
Preferred examples of oral care actives for inclusion in the compositions of the invention include agents for the remineralisation of teeth. The term "remineralisation" in the context of the present invention means the in situ generation of hydroxyapatite on teeth.
A specific example of a suitable agent for the remineralisation of teeth is a mixture of a calcium source and a phosphate source which, when delivered to the teeth results in the in situ generation of hydroxyapatite on teeth.
Illustrative examples of the types of calcium source that may be used in this context (hereinafter termed "remineralising calcium sources") include, for example, calcium phosphate, calcium gluconate, calcium oxide, calcium lactate, calcium glycerophosphate, calcium carbonate, calcium hydroxide, calcium sulphate, calcium carboxymethyl cellulose, calcium alginate, calcium salts of citric acid, calcium silicate and mixtures thereof. Preferably, the remineralising calcium source is calcium silicate. The amount of remineralising calcium source(s) (e.g. calcium silicate) in the composition of the invention typically ranges from 1 to 30%, preferably from 5 to 20% by total weight remineralising calcium source based on the total weight of the oral care composition. Compositions of the present invention may also contain further optional ingredients customary in the art such as anticaries agents, anticalculus agents, buffers, flavouring agents, sweetening agents, colouring agents, opacifying agents, preservatives, antisensitivity agents, antimicrobial agents and the like. Preferably the composition comprising a whitening agent. Suitable whitening agents comprise titanium dioxide, mica and blue dyes/pigments. Mixtures of whitening agents may be used.
Process
A toothpaste was manufactured by the following steps: i) Addition of an anionic surfactant to a polyol and heating to a temperature such that the surfactant completely dissolves in the polyol followed by; ii) addition of other ingredients with the exception of alkali metal salt (phosphate), perfume and flavours; iii) addition of alkali metal salt (phosphate) and allow time for solution to disperse; iv) optionally; v) cooling of the mix to a temperature below the solubility point of the surfactant in polyol; vi) addition of perfumes and flavour; vii) cooling resulting in a structured mix. Constant Shear is present from the start of the process to the end. So the shear does not impact upon the invention but will help surfactants and metal salts to dissolve but their dissolution is mostly influence by temperature. The invention is further illustrated with reference to the following, non-limiting Examples.
EXAMPLES Test formulations were prepared having the ingredients shown in Table 1 below.
All ingredients are expressed by weight percent of the total formulation, and as level of active ingredient, unless otherwise specified. Structured formulation - Surfactant introduced early and dissolved before introduction of alkali metal salts are shown in Table 1 :
Table 1
The following process was used to prepare the Examples: Stage 1 :
Add SLS, calcium silicate to cold glycerol or polyol and then heat from ambient to 60oC or 7oOC - mix for 10 minutes at 60oC to 70oC. Stage 2:
Add SMFP, Sweetener and Titanium dioxide and mix for 10 minutes at 60oC to 70oC.
Stage 3:
Add abrasives particles, calcium phosphate, monosodium phosphate, trisodium phosphate and mix for 20 minutes.
Stage 4:
Cool to 45oC then add flavour, mix for 5 minutes and then cool to discharge the product. Examples of Unstructured Formulation (eg surfactant introduced late or after the source of phosphate) are shown in Table 2.
Table 2
The commonly used process for the unstructured products: Stage 1 :
Add calcium silicate, Sweetener, Titanium dioxide to cold glycerol and then heat from ambient to 60oC or 7oOC - mix for 10 minutes at this temperature. Stage 2:
Add SMFP, Sweetener, monosodium phosphate, trisodium phosphate and mix for 10 minutes at 60oc to 70oC
Stage 3:
Add titanium dioxide, abrasive and mix for 10 min. Stage 4:
Add calcium phosphate and surfactant and mix for 10 min. Stage 5:
Cool to 45°C then add flavour, mix for 5 minutes and then cool to discharge the product.
The viscosity (measured at 20°C) and yield stress of the Examples were measured and are shown in Table 3
Table 3
Viscosity Viscosity Viscosity Yield Stress (Pa.s) (Pa.s) (Pa.s) (Pa) at shear rate at shear rate at shear rate
of 0.001 s"1 of 0.01 s"1 of 0.1 s"1
Example 1 10430 4771 935 1 10 Pa
SLS early
Example A 80 49 31 No Yield Stress
SLS late as unstructured
Example 2 13600 5982 1 106 137 Pa
SLS early
Example B 125 120 78 No Yield Stress
SLS late as unstructured
Example 3 550 381 200 5 Pa
SMCT early
Example C 95 70 48 No Yield Stress
SMCT late unstructured Products made according to the invention (surfactant early and solubilised before introduction of alkali salts to polyol) do not need any extra structuring technologies (such as polymers) in them as these products hold their structure until a certain stress is applied to them - They typically exhibit a yield stress and behave as a toothpaste.
Product made with surfactant added late (which do not comprise structuring polymer) would flow under any stress and in fact would behave as a liquid or a thick slurry. They would therefore need extra structuring technology to achieve toothpaste properties.

Claims

Process for manufacturing a non-aqueous composition comprising the following steps: i) addition of an anionic surfactant selected form the group consisting of , alfa olefin sulfonate, lauryl phosphate, sodium coco sulphate, sodium methyl cocoyl taurate, sodium methyl oleoyl taurate, sodium lauryl sulphate, sodium cocoyl isethionate, disodium lauryl sulfosuccinate, to a polyol at a temperature such that the surfactant completely dissolves in the polyol followed by; ii) addition of an alkali metal phosphate salt; cooling of the mix to a temperature below the solubility point of the surfactant in polyol, the cooling resulting in a structured mix, in which the weight ratio of alkali metal phosphate salt to surfactant is from 1.1 :1 to 10:1 .
Process according to claim 1 in which a perfume and/or flavouring is added after the mix is cooled to a temperature below the solubility point of the surfactant in the polyol.
Process according to claim 1 or claim 2 in which the alkali metal salt is a sodium or potassium salt.
Process according to any preceding claim in which the phosphate is selected from monosodium phosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, sodium pyrophosphate, tetrasodium pyrophosphate, sodium
tripolyphosphate, sodium hexametaphosphate, potassium dihydrogenphosphate, trisodium phosphate, tripotassium phosphate.
5. Process according to claim 4 in which the phosphate is selected from tri sodium phosphate and monosodium phosphate or mixtures thereof.
6. Process according to any preceding claim in which the total level of phosphate salt is form 2 to 10 wt% of the total composition.
7. Process according to any preceding claim in which the polyol is glycerol.
8. Process according to any preceding claim in which the anionic surfactant is
selected from the group consisting of sodium coco sulphate, sodium methyl cocoyl taurate sodium lauryl sulphate (SLS) and mixtures thereof.
9. Process according to any preceding claim in which the weight ratio of phosphate to surfactant is from 1.1.1 to 5.1.
10. Process according to any preceding claim in which the surfactant is heated in the polyol to a temperature of 60 °C.
1 1. Process according to any preceding claim in which perfume or flavouring is added to the mix after step iii) of the process at 45°C or below.
12. Process according to any preceding claim in which the composition is a toothpaste.
13. Process according to any preceding claim in which further ingredients are added to the composition after the dissolution of the surfactant in the polyol (i).
14. Use of surfactant crystals selected from the group consisting of, alfa olefin
sulfonate, lauryl phosphate, sodium coco sulphate, sodium methyl cocoyl taurate, sodium methyl oleoyl taurate, sodium lauryl sulphate, sodium cocoyl isethionate, disodium lauryl sulfosuccinate, to structure a non-aqueous paste comprising polyol and alkali metal phosphate.
EP17780360.8A 2016-10-10 2017-09-28 Process for manufacture of non-aqueous oral care compositions Active EP3522855B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP16193162 2016-10-10
PCT/EP2017/074633 WO2018069054A1 (en) 2016-10-10 2017-09-28 Process for manufacture of non-aqueous oral care compositions

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EP3522855A1 true EP3522855A1 (en) 2019-08-14
EP3522855B1 EP3522855B1 (en) 2021-10-27

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CN (1) CN109890349B (en)
BR (1) BR112019006206B1 (en)
CL (1) CL2019000944A1 (en)
EA (1) EA201990596A1 (en)
PH (1) PH12019500693B1 (en)
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN119894484A (en) * 2022-08-31 2025-04-25 联合利华知识产权控股有限公司 Method for producing non-aqueous composition
CN121263166A (en) * 2023-05-26 2026-01-02 联合利华知识产权控股有限公司 Method for producing non-aqueous composition

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5726612A (en) * 1980-07-24 1982-02-12 Lion Corp Preparation of oral composition
US5254334A (en) * 1992-05-04 1993-10-19 Imaginative Research Associates, Inc. Anhydrous foaming composition containing low concentrations of detergents and high levels of glycerin amd emollients such as oils and esters
US5409706A (en) * 1992-05-04 1995-04-25 Imaginative Research Associates, Inc. Anhydrous foaming composition containing low concentrations of detergents and high levels of glycerin and emollients such as oils and esters
GB9414721D0 (en) 1994-07-21 1994-09-07 Smithkline Beecham Plc Dentifrice composition
CN105342894A (en) * 2015-11-12 2016-02-24 邹文君 Yizao toothpaste added with functional modified composite micromolecule material with high permeability and preparation method of Yizao toothpaste

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CL2019000944A1 (en) 2020-03-20
EA201990596A1 (en) 2019-10-31
EP3522855B1 (en) 2021-10-27
BR112019006206A2 (en) 2019-06-18
PH12019500693B1 (en) 2023-04-26
CN109890349B (en) 2022-06-17
CN109890349A (en) 2019-06-14
PH12019500693A1 (en) 2019-11-04
WO2018069054A1 (en) 2018-04-19
BR112019006206B1 (en) 2022-09-13

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